Process of making salts of ammonia, especially sulfate of ammonia.



0. P. HURFORD.

PROCESS OF MAKING SALTS 0F AMMONIA, ESPECIALLY SULFATE 0F AMMONIA.

AYPLIOATION FILED DEO.12,1908.

940,972. Patented Nov. 23. 1909.

2 SHEETS-SHEET 1.

fi .ww, aim/amalgam.

0. P. HURFORD. PBLOGESS OF MAKING SALTS OFAMMONIA, ESPECIALLY SULFATE 0F AMMONIA.

APYLIOATION FILED D110. 12, 1908.

940,972. Patented N0v.23, 1909.

Z SHEETS-SHEET 2.

I UNITED STATES PnEENT OFFICE.

orrvn i r. Huaronn, or cirrcaso, rumors.

4e cause the nitrogen and hydrogen gases to PROCESS OF MAKING SALTS OF AMMONIA, ESPECIALLY SULFATE 0F AM'iMONIA.

Specification of Letters Intent.

Patented Nov. 23, 1909.

Application filed December 12, 1998, Serial No. 467,125.

; tion.

My invention relates to a method and apparatus for the manufacture of ammonia compounds, particularly sulfate of ammonia.

My method, broadly speaking, consists in causing the chemical union of nitrogen gasand hydrogen gas under the influence of electrical discharges, in the presence of a suitable acid which combines with the ammonia as fast as it is formed to hold the same by forming a com ound of ammonia. Without the presence 0 a third element to hold or fix the'amnionia gas, the latter would be disassociated into its constituent elements of hydrogen and nitrogen by the further action of the electric sparks or dischar es. The percentage of ammonia formed in this way depends upon the length of the electric spark, but it may be stated that usually from two tosix per cent. will be formed. The disassociation of the ammonia into its constituent elements is to the extent of about eighty-six per cent of the ammonia actually formed. It is the object of my invention to revent this disassociation.

- met od is particularly applicable to the manufacture of ammonium sulfate which, as well hown, is one of the best of fertilizers. producing this compound, I

unite under the influence of electric dischar es in ,the presence of sulfuric acid is introduced into the receptadle in sulfuric acid andarnmonia at to form ammonium sulfate, which is then I withdrawn from the which is well of 'my process, id

I have also devised a' orm of apparatus ada ted for the carryi out ough various other orms ofapparatus might be devised for the same urpose. The essence of my invention as process is in no way dependent u n he particular form of apparatus emically at 19,

, Before explaining the details of my proc: ess, I shall describe the form of apparatus which I have shown in the accompanying drawings, where Figure 1 is a detail cross-sectional view of a.form of apparatus which I have devised in this connection, certainof the parts being, for the sake of clearness, shown in full; and Fig. 2, is a detail cross-sectional view of a slightly modified form of apparatus.

The cylindrical receptacle 1 is lined upon the interior thereof with a suitable insulat ing material 2. Projecting into this receptacle is a series of pipes or tubes 4 preferably of insulating material, as for instance, glass. The inner ends of these tubes may be provided with slotted enlargements 5 in the shape of flattened funnels. The slots or openings are indicated. at 6. The tubes 4 are at their outer ends connected to the stand-pipe7, with which they arevin communication. Extending into the receptacle from the opposite side IS a series of'tubes 8 also preferably of insulatin material, and provided at their inner en 5 with slotted enlargements 8, having ends in the shape of flattened funnels 9, similar to the enlar einents on the tubes 4. At their outer en s, the tubes 8 are connected with the stand pipe 10, with which they are in communication. The stand pipe 7, which is closed at the top, is at its other end in communication with a source of hydrogen gas su ply, as indicated. diagrammatically by the arrow 11. Between pipe 12, leading from the gas sup ly, and pipe 13 is a blowerthrough the stand pipe 7. A gage 15 may .be used to indicate'the pressure in the pipe. The stand pipe 10, which is closed at'the top, is at its other end incommunication with a source of nitro on gas supply, as indicated diagrammatica 1y b the arrow 16. Between the pipe 17,1eading rom the source of nitrogen supply, and pipe 18, there is a blower-ar :v nt- .indicated'diagrammatto the blower-arrangementused in ec tion with the other stand pipe The object of the blower arrangement 19 is to maintain the pressure of the gas in the stand pipe 10, practically constant. By r ulating the speed of the blowers in. 14 an 19, the -gases may be kept at the same pressures 15m: rrespective stand p1pes, so'that they will be discharged into the receptacle at. the same pressure. If desirable, valves 20. and '21 may be .used in connection with the tubes 4 and 8 respectively, for the purpose of regulating the supply of gas, orshuttin the-same on.

n the upper portion 0 the receptacle is arranged aperforated partition or screen 22.

.A pipe 23 communicates with the top of the receptacle at 24, for the urpose'of introducing asuitable acid into t e receptacle. As it comes into-contact with the perforated partition 22, the acidis, as it were, broken up into a line spray, in which form it passes through-the receptacle. A valve 242' may be trodes are of course thoroughly insulated .from any metallic as indicated by the msulatin sleeves 27. 1--

arts of the apparatus,

have not deemed it desirab e to show the complete electrical circuit of these electrodes for the reason that it lies w thin the skill of any electrician toconnect tlr e e ectrodes properly in the desired circuit. I ha e merely indicated bythe wires 28 and 29 that the electrodes are to be connected in a suitable electrical circuit, calculated to cause the passage of sparks between the electrodes 25 and 26 inthe receptacle. The amount of, voltage necessary to produce such arking is purely a matter of mathematic'a calculation, depending among other thin upon the distance between the electro es used. For instance, in certain cases 50,000

volts might be sufiicient to produce the nec essary discharges, while in other instances a higher. voltage mightbe necessary.

With this descrlption ofia. form of apparatus adapted to carry, out my process, 'I shall now describe the various steps-of my process: The nitrogen gas is introduced into the receptacle through tubes 8, while the hydro en gas is introducedthrough the oppos tely situated pi es 4. It will be notlced that in Fig. 1 tie pipes 4 and 8 are arranged in stag ering relation while" in the modification s own in Fig.2, they are The precise arrangement of the supply tubes is more or less of a mechanical detail depending upon the precise arran ement of the electrodes. With the electro es garrangell as Fi 1, a wider discharges y arranging the supply tubes in a s'ta'ggering'relation. In Fi 2 the electrodes 25' and 26' are substantially in alinement, each pair ofelectrodes being arranged [charges take place with the nitrogen and h in which the gases unite,

it is not, of course, absolutely necessary that mation,

ath is provided 'for' the electric betweena pair of supply pipes. the number'pf pairs of electrodes as well asthe number of supply pipes ma Of course,

be varied. I

according ,to circumstances. As e ectl'ical disdrogen gases streaming into the receptac e, the following chemicalreactiontakes placer This, interpreted means'thatone: volume of nitrogen gas comb hydrogen gas to form twovolumes of ammonia' gas; On account of this-proportion, v the stand pipe 7- through which the-hydrogen passes has a volume approximately three tlmes that of the stand pirie 10, through which the nitrogen passes. he supply tubes 4 have a crosssectional area a proximately three, times that of the supp y tubes 8.' The result of this arrangement isthat approximately three times -as much hydrogen 15 introduced ines with three volumes of into the receptacle as nitrogen. .Although the gases be introduced into the receptacle, they will combine in norother proportion than that above indicated,- that is to say, in the proportionof three volumes of hydro-' gen-to one volume-of nitrogen. However unless, some third element be introduced into the receptacle to hold-.01: fix the ammonia gas, the latter will, under the im flue'nce of the continued electric discharges, be disassociated into the elements nitrogen and hydro en. "For this reason, I introduce a, suitab e acid through the plpe 23 "the par-' ticular kind of acid used d'epenclin is desired to obtain. In the manufacture. of sulintc ofnmmouia, "sulfuric acid is "introduccd. If some other acid", for instance, llyd'rtxchloric ucith be used, the. resulting product would be ammonium chlorid. As-

suming that it is desired to make ammonia sulfate, snlfuric'acid is introduced through the pipe 23, and as it falls'upon the screen or perforated partition 22 it will be scattered, as it were, and pass through the screen into the receptacle 1n the form of a fine spray or vapor. The spray or vapor of sulfuric acid coming into contact with theammonia gas, at the very instant of its for- I results in the following chemical reaction: v

upon the purticulu" ammonium product w nch 1t sulfate, or sulfate ofammonia as it is also called. This liquid is led out. of the tacle 'throu h the discharge bottom of he receptacle. case it is'found recap. pipe 30'at te that the ammonia sulfate contains an excess of sulfuric acid, it may be sub ected to treatmentfor the neutralization of the sulfuric acid by some alkali. If it is desired to thus subject the ammonium sulfate to this further treatment, it may be led out the chemical union of nitrogen gas and hydrogen gas, discharges in the presence of an acid wh ch will hold the ammonia gas by combining with it to form an ammonium compound. The various attendant details in the carr ing out of the process may be varied and naturally would be varied, under varying circumstances. For this reason, I have not attempted nor found it necessary to specify dimensions of the apparatus, or the part1cular manner in which the electrodesshould be arranged in the receptacle. found it necessary to describe the kind of electrical energy with which the discharge electrodes are connected or any of the circuit arrangements. These, as above stated, are details that are well understood by those skilled in the electrical art.

Having thus described my invention, what 1 claim" as new and desire to secure by Letters Patent of the United States is:-

l. The process of producing sulfate of ammonia which consists in causing nitrogen gas and hydrogen gas to unite under the influence of electric discharges to form ammonia gas, and subjecting the ammonia gas as fast as it is formed to the action of su1 furic acid, whereby sulfate of ammonia is formed.

2. The process of producing sulfate of ammonia which consists in leading nitrogen gas and hydrogen gas into a closed recepta- (-le, causing the mixed gases to unite in said receptacle under the influence of electric discharges to form ammonia'gas,simultaneously'introducing sulfuric acid into the receptacle, whereby the ammonia gas combines with the sulfuric acid to form sulfate of ammonia, and withdrawing the sulfate of ammonia thus formed.

3. The process of producing sulfate of ammonia which consists in causing nitrogen gas and hydrogen gas to unite under the influence of electric discharges to form ammonia gas in the resence of sulfuric acid which combines with the ammonia gas to form sulfate of ammonia.

4. The process of producing sulfate of ammonia which consists in causing nitrogen gas and hydrogen gas to unite under the influence of electric discharges to form ammonia gas, while causing a spray of sulfuric acid to pass through the receptacle, whereby the ammonia gas combines with the sulfuric acid to form sulfate of ammonia, and withdrawing the sulfate of ammonia from the receptacle.

under the influence of electri'c' Nor have I 5. The process of producin sulfate of ammonia, which consists in lea mg nitrogen gas and hydrogen gas. separately into a closed receptacle, approximately in the proportion of one volume of nitrogen to t ree volumes of hydrogen, causing the mixed gases to unite under the influence of electric discharges to form ammonia gas, while causing a. spray'ofsulfuric acid to pass through the receptacle, whereby the ammonia gas combines with the sulfuric acid to form sulfate of ammonia and withdrawing the sulfate of ammonia from the receptacle.

6. The process of producing salts of mm monia which consists in causing nitrogen gas and hydrogen gas to unite under the influence of electric discharges to form ammonia gas in the presence of an acid which combines with the ammonia gas to form a salt of ammonia.

7. The process of producing sulfate 0 ammonia which consists in leading hydrogen 'gas and nitrogen gas separately into a receptacle where they become mixed, causing the mixed gases to unite in the receptacle under the influence of electric discharges to form ammonia gas, and subjecting the ammonia gas as fast as it is formed to the action of sulfuric acid to combine with the ammonia gas to form sulfate of ammonia.

8. The process 'of producing sulfate of annnonia-which consists in leading hydrogen gas and nitrogen gas se arately into a receptacle from opposite si es thereof hereby the gases become mixed, causing the mixed gases to unite in the receptacle under the influence of electric discharges'to form ammonia gas, and subjecting the ammonia gas as fast as it is formed to the action of sulfuric acid to combine with the ammonia gas to form sulfate of ammonia.

9. The process of producing sulfate of ammonia which consists in leading hydrogen gas and nitrogen gas into a receptacle, causing the mixed ases to unite in the receptacle under the in uence of electric dischar es to form ammonia gas, in the presence of a descending spray of sulfuric acid, which combines with the ammonia gas as fast as it is formed and carries it in the form of sol- I fate of ammonia to the bottom of the receptacle, and withdrawing the sulfate of ammonia thus formed.

10. In an apparatus of the kind described, the combination of a closed receptacle, a series of tubes extending into said receptacle from opposite sides thereof and arranged to be connected with a source of gas supply, said tubes having openings for introducing gases into the receptacle, electrodes extending into thereceptacle and adapted to be connected to a suitable source of current supply to produce discharges between said electrodes, whereby the gases'in the receptacle are caused to unite to form a compound,

mean s for introducing a suitable substance into the receptacle during the discharges to act upon the com ound ormed, and'means for withdrawing e product.

11. In an apparatus of the kind described,.

.the COII'Ibilltl-tlOIl of a closed receptacle, a pair of pi es associated therewith'and 'connected eac with a source of gas s u ply, a

d pipes fsries of tubes extending from sai at their.

into the-receptacle,-said tubes bein inner ends provided with-openings or introfducing the gases into the reeeptacle, elec- U trodes extending into the receptacle and compound, means udapted to-be connected to a suitable source of current supply produce discharges be tween said electrodes, whereby the gases in the receptacle are caused ,to unite to form a and means "for wlthdrawin t e product.-

@ 12. In an apparatus of]; e kind described;

v the combination of a closedjrece tacle having an insulatin liningupon e interior thereof, a pan-o pipes associated therewith v terlal extendin I forintroduc'ing a spray of ac d into the receptacle durin the discharges to act upon the comgoun formed, 1

endsprovided with enlargementsi haning 30 openings for introducing'the gase'smto the v receptacle, electrodes extending into the receptacle and adapted to be connected to a sultable source of current suppl to produce discharges between said electro es, whereby 85 'the ases in the receptacle 7 are caused to uilcite to form a compound, a perforated partition in vthe upper part ofthe rece tacle for introducing a spray of acid into e receptacle-during the discharges to act upon) the compound vformed, and means for Wltll':

- drawing the product.

In witness. whereof, I hereunto subscribe T OLIVER Pi HURFORD. I Witnesses: p 1

LEONARD 'W. NQVKANDER;

A; A. THOMAS.

gas t.

my name 'this 9th day of DecemberA, D. 90s. 

